JPWO2019004255A1 - エチレン−ビニルアルコール系共重合体組成物、ペレット群および多層構造体 - Google Patents
エチレン−ビニルアルコール系共重合体組成物、ペレット群および多層構造体 Download PDFInfo
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- JPWO2019004255A1 JPWO2019004255A1 JP2018534184A JP2018534184A JPWO2019004255A1 JP WO2019004255 A1 JPWO2019004255 A1 JP WO2019004255A1 JP 2018534184 A JP2018534184 A JP 2018534184A JP 2018534184 A JP2018534184 A JP 2018534184A JP WO2019004255 A1 JPWO2019004255 A1 JP WO2019004255A1
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- Japan
- Prior art keywords
- ethylene
- evoh resin
- vinyl alcohol
- evoh
- resin composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 229920000219 Ethylene vinyl alcohol Polymers 0.000 title claims abstract description 289
- 239000000203 mixture Substances 0.000 title claims abstract description 21
- 239000008188 pellet Substances 0.000 title claims description 35
- 239000004715 ethylene vinyl alcohol Substances 0.000 claims abstract description 279
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000005977 Ethylene Substances 0.000 claims abstract description 79
- 150000002506 iron compounds Chemical class 0.000 claims abstract description 44
- 229920001577 copolymer Polymers 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- RZXDTJIXPSCHCI-UHFFFAOYSA-N hexa-1,5-diene-2,5-diol Chemical compound OC(=C)CCC(O)=C RZXDTJIXPSCHCI-UHFFFAOYSA-N 0.000 claims abstract 20
- 238000002156 mixing Methods 0.000 claims description 25
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000004040 coloring Methods 0.000 abstract description 17
- UFRKOOWSQGXVKV-UHFFFAOYSA-N ethene;ethenol Chemical compound C=C.OC=C UFRKOOWSQGXVKV-UHFFFAOYSA-N 0.000 description 259
- 229920005989 resin Polymers 0.000 description 199
- 239000011347 resin Substances 0.000 description 199
- 239000011342 resin composition Substances 0.000 description 105
- 238000000034 method Methods 0.000 description 73
- 239000010410 layer Substances 0.000 description 55
- -1 polypropylene Polymers 0.000 description 31
- 229920001567 vinyl ester resin Polymers 0.000 description 21
- 239000002585 base Substances 0.000 description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 238000010438 heat treatment Methods 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
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- 238000007127 saponification reaction Methods 0.000 description 15
- 229920006223 adhesive resin Polymers 0.000 description 14
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- 230000000694 effects Effects 0.000 description 14
- 150000003839 salts Chemical class 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- 229910052742 iron Inorganic materials 0.000 description 11
- 238000002844 melting Methods 0.000 description 11
- 230000008018 melting Effects 0.000 description 11
- 229920005672 polyolefin resin Polymers 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000000465 moulding Methods 0.000 description 9
- 239000013585 weight reducing agent Substances 0.000 description 9
- 239000004743 Polypropylene Substances 0.000 description 8
- 125000004432 carbon atom Chemical group C* 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000001125 extrusion Methods 0.000 description 8
- 229920001155 polypropylene Polymers 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 235000013305 food Nutrition 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000155 melt Substances 0.000 description 7
- 239000000178 monomer Substances 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000006096 absorbing agent Substances 0.000 description 6
- 238000000071 blow moulding Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 235000014113 dietary fatty acids Nutrition 0.000 description 6
- 229930195729 fatty acid Natural products 0.000 description 6
- 239000000194 fatty acid Substances 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229920005992 thermoplastic resin Polymers 0.000 description 6
- 239000004711 α-olefin Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000314 lubricant Substances 0.000 description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 5
- 239000005022 packaging material Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 229920000098 polyolefin Polymers 0.000 description 5
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 4
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 239000003905 agrochemical Substances 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
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- 238000010030 laminating Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920001225 polyester resin Polymers 0.000 description 3
- 229920002223 polystyrene Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000004709 Chlorinated polyethylene Substances 0.000 description 2
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- 239000004278 EU approved seasoning Substances 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- 240000008415 Lactuca sativa Species 0.000 description 2
- 244000294411 Mirabilis expansa Species 0.000 description 2
- 235000015429 Mirabilis expansa Nutrition 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 2
- 150000004056 anthraquinones Chemical class 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 235000013361 beverage Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 description 2
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- 229920005676 ethylene-propylene block copolymer Polymers 0.000 description 2
- 235000021107 fermented food Nutrition 0.000 description 2
- 229960004887 ferric hydroxide Drugs 0.000 description 2
- 229960002089 ferrous chloride Drugs 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 235000011194 food seasoning agent Nutrition 0.000 description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 238000009998 heat setting Methods 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
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- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229920000554 ionomer Polymers 0.000 description 2
- 150000002505 iron Chemical class 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910000398 iron phosphate Inorganic materials 0.000 description 2
- 229910000358 iron sulfate Inorganic materials 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 2
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 235000010746 mayonnaise Nutrition 0.000 description 2
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- QLZJUIZVJLSNDD-UHFFFAOYSA-N 2-(2-methylidenebutanoyloxy)ethyl 2-methylidenebutanoate Chemical class CCC(=C)C(=O)OCCOC(=O)C(=C)CC QLZJUIZVJLSNDD-UHFFFAOYSA-N 0.000 description 1
- HKUDVOHICUCJPU-UHFFFAOYSA-N 2-(2-methylprop-2-enoylamino)propane-1-sulfonic acid Chemical compound OS(=O)(=O)CC(C)NC(=O)C(C)=C HKUDVOHICUCJPU-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
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- HOVLEIUJGCUOMI-UHFFFAOYSA-N 2-(butanoyloxymethyl)prop-2-enyl butanoate Chemical compound CCCC(=O)OCC(=C)COC(=O)CCC HOVLEIUJGCUOMI-UHFFFAOYSA-N 0.000 description 1
- MVYVKSBVZFBBPL-UHFFFAOYSA-N 2-(prop-2-enoylamino)propane-1-sulfonic acid Chemical compound OS(=O)(=O)CC(C)NC(=O)C=C MVYVKSBVZFBBPL-UHFFFAOYSA-N 0.000 description 1
- DIBCJRYCOGXPAM-UHFFFAOYSA-N 2-(propanoyloxymethyl)prop-2-enyl propanoate Chemical compound CCC(=O)OCC(=C)COC(=O)CC DIBCJRYCOGXPAM-UHFFFAOYSA-N 0.000 description 1
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- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
Description
<EVOH樹脂組成物>
本発明のEVOH樹脂組成物は、エチレン含有量が異なる2種以上のEVOH樹脂を有するEVOH樹脂(A)を主成分とし、さらに鉄化合物(B)を含有するものである。本発明のEVOH樹脂組成物は、ベース樹脂がEVOH樹脂(A)である。すなわち、EVOH樹脂組成物におけるEVOH樹脂(A)の含有量は、通常70重量%以上であり、好ましくは80重量%以上であり、より好ましくは90重量%以上であり、特に好ましくは95重量%以上である。以下、各成分について順に説明する。
EVOH樹脂は、通常、エチレンとビニルエステル系モノマーとの共重合体であるエチレン−ビニルエステル系共重合体をケン化させることにより得られる樹脂であり、非水溶性の熱可塑性樹脂である。そして、本発明で用いるEVOH樹脂(A)は、エチレン含有量が異なる2種以上のEVOH樹脂を有するものである。なお、上記EVOH樹脂のエチレン含有量は、ISO14663に基づいて測定した値を意味する。
本発明のEVOH樹脂組成物は、上記エチレン含有量が異なる2種以上のEVOH樹脂を有するEVOH樹脂(A)に加え鉄化合物(B)を含有し、かつ鉄化合物(B)の配合量が特定微量であることを特徴とする。本発明のEVOH樹脂組成物は、上記のような構成を有するため、着色を抑制することができ、熱安定性に優れる。
本発明のEVOH樹脂組成物には、EVOH樹脂(A)以外の熱可塑性樹脂を、本発明の効果を阻害しない範囲(例えば、EVOH樹脂組成物の通常30重量%以下、好ましくは20重量%以下、特に好ましくは10重量%以下)にて含有することができる。
また、本発明のEVOH樹脂組成物には、本発明の効果を阻害しない範囲において、一般にEVOH樹脂に配合する配合剤が含有されていてもよい。例えば、無機複塩(例えば、ハイドロタルサイト等)、可塑剤(例えば、エチレングリコール、グリセリン、ヘキサンジオール等の脂肪族多価アルコール等)、酸素吸収剤[例えば、アルミニウム粉、亜硫酸カリウム、光触媒酸化チタン等の無機系酸素吸収剤;アスコルビン酸、さらにその脂肪酸エステルや金属塩等、ハイドロキノン、没食子酸、水酸基含有フェノールアルデヒド樹脂等の多価フェノール類、ビス−サリチルアルデヒド−イミンコバルト、テトラエチレンペンタミンコバルト、コバルト−シッフ塩基錯体、ポルフィリン類、大環状ポリアミン錯体、ポリエチレンイミン−コバルト錯体等の含窒素化合物と鉄以外の遷移金属との配位結合体、テルペン化合物、アミノ酸類とヒドロキシル基含有還元性物質の反応物、トリフェニルメチル化合物等の有機化合物系酸素吸収剤;窒素含有樹脂と鉄以外の遷移金属との配位結合体(例えば、メタキシレンジアミン(MXD)ナイロンとコバルトとの組合せ)、三級水素含有樹脂と鉄以外の遷移金属とのブレンド物(例えば、ポリプロピレンとコバルトとの組合せ)、炭素−炭素不飽和結合含有樹脂と鉄以外の遷移金属とのブレンド物(例えば、ポリブタジエンとコバルトとの組合せ)、光酸化崩壊性樹脂(例えば、ポリケトン)、アントラキノン重合体(例えば、ポリビニルアントラキノン)等や、さらにこれらの配合物に光開始剤(ベンゾフェノン等)や過酸化物捕捉剤(市販の酸化防止剤等)や消臭剤(活性炭等)を添加したもの等の高分子系酸素吸収剤]、熱安定剤、光安定剤、紫外線吸収剤、着色剤、帯電防止剤、界面活性剤(ただし、滑剤として用いるものを除く)、抗菌剤、アンチブロッキング剤、充填材(例えば、無機フィラー等)等を配合してもよい。なかでも、着色を抑制する観点から、酸素吸収剤が好ましく、特にはテルペン化合物が好ましく用いられる。これらの化合物は、単独でもしくは2種以上併せて用いることができる。
本発明のEVOH樹脂組成物は、エチレン含有量が異なるEVOH樹脂を混合して、EVOH樹脂(A)を製造する工程、EVOH樹脂またはEVOH樹脂(A)に鉄化合物(B)を含有させる工程を経ることにより製造することができる。
EVOH樹脂組成物ぺレットの乾燥前重量(W1)を電子天秤にて秤量し、150℃の熱風乾燥機中で5時間乾燥させ、デシケーター中で30分間放冷後の重量(W2)を秤量し、下記式より算出する。
含水率(重量%)=[(W1−W2)/W1]×100
重量減少割合(%)=[(加熱前重量−加熱後重量)/加熱前重量]×100
本発明の多層構造体は、上記本発明のEVOH樹脂組成物からなる層を備えるものである。本発明のEVOH樹脂組成物からなる層(以下、「EVOH樹脂組成物層」と称する。)は、本発明のEVOH樹脂組成物以外の熱可塑性樹脂を主成分とする他の基材(以下、「基材樹脂」と称する。)と積層することで、さらに強度を付与したり、EVOH樹脂組成物層を水分等の影響から保護したり、他の機能を付与することができる。
なお、例中「部」とあるのは、断りのない限り重量基準を意味する。
・EVOH樹脂(A1):エチレン構造単位の含有量の平均値が29モル%、ケン化度99.6モル%、MFR3.9g/10分(210℃、荷重2160g)のエチレン−ビニルアルコール共重合体
・EVOH樹脂(A2):エチレン構造単位の含有量の平均値が44モル%、ケン化度99.6モル%、MFR3.3g/10分(210℃、荷重2160g)のエチレン−ビニルアルコール共重合体
上記EVOH樹脂(A1)およびEVOH樹脂(A2)のペレットを粉砕したサンプル0.5gを赤外線加熱炉で灰化処理(酸素気流中650℃、1時間)し、灰分を酸溶解して純水で定容したものを試料溶液とした。この溶液を下記のICP−MS(Agilent Technologies社製 ICP質量分析装置 7500ce型)を用いて標準添加法で測定した。その結果、鉄化合物(B)の含有量は、共に金属換算にて0ppmであった。
上記EVOH樹脂(A1)のペレット80部と、EVOH樹脂(A2)のペレット20部とをドライブレンドすることによってEVOH樹脂(A)を得た。
実施例1において、リン酸鉄(III)n水和物の配合量を0.00034部(EVOH樹脂組成物の重量あたり金属換算にて1ppm)に変更した以外は、実施例1と同様にして実施例2のEVOH樹脂組成物およびその粉砕物を得た。
実施例1において、リン酸鉄(III)n水和物の配合量を0.0034部(EVOH樹脂組成物の重量あたり金属換算にて10ppm)に変更した以外は、実施例1と同様にして比較例1のEVOH樹脂組成物およびその粉砕物を得た。
実施例1において、リン酸鉄(III)n水和物を配合しなかった以外は、実施例1と同様にして比較例2のEVOH樹脂組成物およびその粉砕物を得た。
上記で得られたEVOH樹脂組成物の粉砕物を、空気雰囲気下のオーブン内で150℃5時間加熱した。加熱後の粉砕品について、ビジュアルアナライザー IRIS VA400(Alpha mos社製)にて、色番号「3819」(R:232、G:232、B:184)が占める割合を評価した。色番号「3819」は、黄色味を有する色であり、この割合が大きいほど、加熱後のサンプルが黄色く着色していることを意味する。
上記で得られたEVOH樹脂組成物の粉砕物を5mg用い、熱重量測定装置(Perkin Elmer社製、Pyris 1 TGA)により、窒素雰囲気下、気流速度:20mL/分、温度:230℃、時間:1時間の条件下での加熱前後の重量から下記式より、重量減少割合を算出した。
重量減少割合(%)=[(加熱前重量−加熱後重量)/加熱前重量]×100
得られた重量減少割合の小数点第2位を四捨五入し、下記の評価基準に基づいて、熱安定性を評価した。
A:0.9% 熱安定性に特に優れる
B:0.8%、または、1.0% 熱安定性に非常に優れる
C:0.7%、または、1.1% 熱安定性に優れる
D:0.6% 熱安定性に劣る
E:〜0.5%、または、1.2%以上〜 熱安定性に非常に劣る
Claims (6)
- エチレン構造単位の含有量が異なる2種以上のエチレン−ビニルアルコール系共重合体を有するエチレン−ビニルアルコール系共重合体(A)と鉄化合物(B)とを含有するエチレン−ビニルアルコール系共重合体組成物であって、上記鉄化合物(B)の含有量がエチレン−ビニルアルコール系共重合体組成物の重量あたり、金属換算にて0.01〜5ppmであることを特徴とするエチレン−ビニルアルコール系共重合体組成物。
- 上記エチレン構造単位の含有量が異なる2種以上のエチレン−ビニルアルコール系共重合体を有するエチレン−ビニルアルコール系共重合体(A)における、最もエチレン構造単位の含有量が高いエチレン−ビニルアルコール系共重合体と、最もエチレン構造単位の含有量が低いエチレン−ビニルアルコール系共重合体とのエチレン構造単位の含有量の差が、2モル%以上であることを特徴とする請求項1記載のエチレン−ビニルアルコール系共重合体組成物。
- 上記エチレン構造単位の含有量が異なる2種以上のエチレン−ビニルアルコール系共重合体を有するエチレン−ビニルアルコール系共重合体(A)が、エチレン構造単位の含有量が35モル%未満のエチレン−ビニルアルコール系共重合体(A1)と、エチレン構造単位の含有量が35モル%以上のエチレン−ビニルアルコール系共重合体(A2)を少なくとも有することを特徴とする請求項1または2記載のエチレン−ビニルアルコール系共重合体組成物。
- 上記エチレン構造単位の含有量が35モル%以上のエチレン−ビニルアルコール系共重合体(A2)に対する上記エチレン構造単位の含有量が35モル%未満のエチレン−ビニルアルコール系共重合体(A1)の重量配合比率が、エチレン構造単位の含有量が35モル%未満のエチレン−ビニルアルコール系共重合体(A1)/エチレン構造単位の含有量が35モル%以上のエチレン−ビニルアルコール系共重合体(A2)=90/10〜10/90であることを特徴とする請求項3記載のエチレン−ビニルアルコール系共重合体組成物。
- 請求項1〜4のいずれか一項に記載のエチレン−ビニルアルコール系共重合体組成物からなることを特徴とするペレット群。
- 請求項1〜4のいずれか一項に記載のエチレン−ビニルアルコール系共重合体組成物からなる層を備えることを特徴とする多層構造体。
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US11124642B1 (en) | 2021-03-18 | 2021-09-21 | Chang Chun Petrochemical Co., Ltd. | Ethylene-vinyl alcohol copolymer composition with improved oxygen barrier properties |
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